1,2-diiodo-3,3-dimethylbut-1-ene was synthesized used 3,3-dimethylbut-1-yne as the initial materials and Ce2(SO4)3 as catalyst in H2O.Then 5,5-dimethyl-1-(o-aminophenyl)-1,3-hexadiyne was synthesized from 1,2-diiodo-3...1,2-diiodo-3,3-dimethylbut-1-ene was synthesized used 3,3-dimethylbut-1-yne as the initial materials and Ce2(SO4)3 as catalyst in H2O.Then 5,5-dimethyl-1-(o-aminophenyl)-1,3-hexadiyne was synthesized from 1,2-diiodo-3,3-dimethylbut-1-ene and 2-ethynylaniline by cross-coupling rection in the presence of Pd(OAc)2 and CuI.The total yield was 68.7 %.The structure was characterized by NMR and MS spectrum.展开更多
The geometry and the potential curve of thermal decomposition for 1,1′dimethyl-5,5′-azotetraol (1-DMAT) are calculated by ab initio quantum chemistry method. The structural characteristics and decomposition mechanis...The geometry and the potential curve of thermal decomposition for 1,1′dimethyl-5,5′-azotetraol (1-DMAT) are calculated by ab initio quantum chemistry method. The structural characteristics and decomposition mechanism are carefully studied. It is found that the terrazzo ring satisfies 4n+2 rule and it is a conjugated π-system for 1-DMAT. The azotetrazol has aromatic characteristic and its thermal decomposition can proceed in two steps: ring opening and separation N2. The activation energies of the two steps are 243.5kJ/mol and 64.01kJ/mol, respectively. The ring opening is the rate-controlling step.展开更多
以草酸与氨基胍碳酸氢盐为原料,经脱水成环、重氮化取代、氧化、中和反应合成了不敏感含能材料1,1′-二羟基-3,3′-二硝基-5,5′-联-1,2,4-三唑二羟胺盐(MAD-X1),总收率为41.2%,采用红外光谱、1 H NMR、13 C NMR及元素分析对产物的结构...以草酸与氨基胍碳酸氢盐为原料,经脱水成环、重氮化取代、氧化、中和反应合成了不敏感含能材料1,1′-二羟基-3,3′-二硝基-5,5′-联-1,2,4-三唑二羟胺盐(MAD-X1),总收率为41.2%,采用红外光谱、1 H NMR、13 C NMR及元素分析对产物的结构进行了表征。探讨了一锅法合成中间体5,5′-二氨基-3,3′-联-1,2,4-三唑(DABT)的机理及亚硝酸钠与硫酸摩尔比对重氮化取代反应收率的影响,对MAD-X1的热性能进行了分析,用NASA-CEA程序计算了MAD-X1-CMDB推进剂的能量特性。结果表明,采用一锅法合成DABT,周期短、收率高(75.1%),亚硝酸钠与硫酸的最佳摩尔比为2.4∶1,酸化试剂为浓盐酸,MAD-X1的热分解峰温度为248.7℃;MAD-X1-CMDB推进剂的理论比冲和特征速度分别为2 449.6N·s/kg和1 540.7m/s。展开更多
文摘1,2-diiodo-3,3-dimethylbut-1-ene was synthesized used 3,3-dimethylbut-1-yne as the initial materials and Ce2(SO4)3 as catalyst in H2O.Then 5,5-dimethyl-1-(o-aminophenyl)-1,3-hexadiyne was synthesized from 1,2-diiodo-3,3-dimethylbut-1-ene and 2-ethynylaniline by cross-coupling rection in the presence of Pd(OAc)2 and CuI.The total yield was 68.7 %.The structure was characterized by NMR and MS spectrum.
基金Sponsored by National Basic Research Program of China Through the Grant ( 2004CB217802 )Educational Committee of Beijing(XK114140479)
文摘The geometry and the potential curve of thermal decomposition for 1,1′dimethyl-5,5′-azotetraol (1-DMAT) are calculated by ab initio quantum chemistry method. The structural characteristics and decomposition mechanism are carefully studied. It is found that the terrazzo ring satisfies 4n+2 rule and it is a conjugated π-system for 1-DMAT. The azotetrazol has aromatic characteristic and its thermal decomposition can proceed in two steps: ring opening and separation N2. The activation energies of the two steps are 243.5kJ/mol and 64.01kJ/mol, respectively. The ring opening is the rate-controlling step.
文摘以草酸与氨基胍碳酸氢盐为原料,经脱水成环、重氮化取代、氧化、中和反应合成了不敏感含能材料1,1′-二羟基-3,3′-二硝基-5,5′-联-1,2,4-三唑二羟胺盐(MAD-X1),总收率为41.2%,采用红外光谱、1 H NMR、13 C NMR及元素分析对产物的结构进行了表征。探讨了一锅法合成中间体5,5′-二氨基-3,3′-联-1,2,4-三唑(DABT)的机理及亚硝酸钠与硫酸摩尔比对重氮化取代反应收率的影响,对MAD-X1的热性能进行了分析,用NASA-CEA程序计算了MAD-X1-CMDB推进剂的能量特性。结果表明,采用一锅法合成DABT,周期短、收率高(75.1%),亚硝酸钠与硫酸的最佳摩尔比为2.4∶1,酸化试剂为浓盐酸,MAD-X1的热分解峰温度为248.7℃;MAD-X1-CMDB推进剂的理论比冲和特征速度分别为2 449.6N·s/kg和1 540.7m/s。
